Professional Documents
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Rectificacion Tequila
Rectificacion Tequila
Communication
Innovation in Continuous Rectification for
Tequila Production
Estarrón-Espinosa Mirna, Ruperto-Pérez Mariela, Padilla-de la Rosa José Daniel * and
Prado-Ramírez Rogelio *
Centro de Investigación y Asistencia en Tecnología y Diseño del Estado de Jalisco (CIATEJ),
Av. Normalistas No. 800, C.P. 44720 Guadalajara, Jalisco, Mexico; mestarron@ciatej.mx (E.-E.M.);
mruperto11@gmail.com (R.-P.M.)
* Correspondence: jdpadilla@ciatej.mx (P.-d.l.R.J.D.); rprado@ciatej.mx (P.-R.R.); Tel.: +33-33455200 (P.-d.l.R.J.D.)
Received: 23 March 2019; Accepted: 6 May 2019; Published: 14 May 2019
Abstract: In this study, a new process of continuous horizontal distillation at a pilot level is presented.
It was applied for the first time to the rectification of an ordinario fraction obtained industrially.
Continuous horizontal distillation is a new process whose design combines the benefits of both
distillation columns, in terms of productivity and energy savings (50%), and distillation stills in batch,
in terms of the aromatic complexity of the distillate obtained. The horizontal process of continuous
distillation was carried out at the pilot level in a manual mode, obtaining five accumulated fractions
of distillate that were characterized by gas chromatography (GC-FID). The tequila obtained from the
rectification process in this new continuous horizontal distillation process complies with the content
of methanol and higher alcohols regulated by the Official Mexican Standard (NOM-006-SCFI-2012).
Continuous horizontal distillation of tequila has potential energy savings of 50% compared to the
traditional process, besides allowing products with major volatile profiles within the maximum limits
established by the regulation for this beverage to be obtained.
1. Introduction
Tequila is a traditional Mexican alcoholic beverage recognized around the world. It is obtained
from distillation of the fermented juice of the Agave tequilana Weber blue variety. The production
process consists of five stages: cooking, grinding, fermentation, distillation, and resting or aging [1].
According to the percentage of sugars belonging to agave used in the production of Tequila, it can
be classified as one of the following categories: Tequila and Tequila 100% Agave [2]. In the case of
Tequila, 51% of the total sugars in the fermentation process must belong to agave, and the rest of
the sugars may be obtained from other sources [3]. The Tequila aroma depends on the amount and
type of volatile compounds present [4]. Tequila’s composition is very complex. Different volatile
compounds have been reported as responsible for the sensorial characteristics of tequila, among
which the most important are alcohols, esters, terpenes, fatty acids, aldehydes, ketones, furans,
sulphur compounds, lactones, and phenols [4,5]. This composition is affected by each of the stages of
its production process, where the distillation process plays an important role. Based on the Official
Mexican Standard regulating tequila composition, the maximum permissible concentration of methanol
is 300 mg/100 mL of anhydrous alcohol, while for higher alcohols, it is 500 mg/100 mL of anhydrous
alcohol [3]. The alcohol concentrations of tequila can be regulated during the distillation process.
Most spirits’ production processes use either batch distillation columns or alembics [6]. The latter
are the most frequently used in small-scale production facilities. In these systems, three cuts (head, heart,
and tail) are collected sequentially; high-quality spirits are produced from the heart cut. Even though
Most
Processes 2019,spirits’
7, 283 production processes use either batch distillation columns or alembics [6]. The latter
2 of 8
are the most frequently used in small-scale production facilities. In these systems, three cuts (head,
heart, and tail) are collected sequentially; high-quality spirits are produced from the heart cut. Even
the operation
though of alembics
the operation of isalembics
relativelyissimple compared
relatively simpletocompared
batch distillation
to batch columns, it involves
distillation columns,many it
uncontrolled and unmeasured disturbances that generate variability
involves many uncontrolled and unmeasured disturbances that generate variability in the in the composition of the final
product [7]. Tequila
composition is obtained
of the final productafter two consecutive
[7]. Tequila is obtained differential
after two distillations
consecutivein pot stills [1].
differential The first
distillations
one, stripping, allows a product called ordinario
in pot stills [1]. The first one, named stripping, allows a product called ordinario to be obtained,20–30%
named to be obtained, whose ethanol content is whose
in volume.
ethanol The second
content is 20–30%one,in named
volume.rectification,
The second consists of distilling
one, named the ordinario
rectification, againofand
consists obtaining
distilling the
three products:
ordinario head,
again and tail, and three
obtaining heart,products:
the latter of which
head, tail,has
andanheart,
ethanolthecontent
latter ofclose to 55%
which in volume,
has an ethanol
which
contentbasically
close to constitutes
55% in volume, a tequila
whichbeverage
basically[8].constitutes a tequila beverage [8].
The use of batch distillation columns results in a higher productivity and higher efficiency of
ethanol recovery compared to the traditional batch process, but a lower presence of compound compound
complexity in the Tequila product
Tequila product [9]. [9].
Recently, innovations have emerged in the distillation area focused on energy reduction,
consumption,
consumption,and andprocess
processtime time[10–12].
[10–12].AA new
new patented
patented technology,
technology,called Continuous
called ContinuousDistillation [13],
Distillation
has been shown to be more efficient and more cost-effective than the traditional
[13], has been shown to be more efficient and more cost-effective than the traditional process. process. Continuous
horizontal
Continuous distillation
horizontal combines the distillation
distillation combines the columns and batch
distillation distillation
columns process.
and batch This system
distillation has
process.
reduced the energy consumption by 50% based on a study where citrus essential
This system has reduced the energy consumption by 50% based on a study where citrus essential oils oils were obtained [14].
Currently,
were obtainedan equipment prototype
[14]. Currently, of continuous
an equipment distillation
prototype has been built,
of continuous which has
distillation consists
beenofbuilt,
five
stages, built in of
which consists stainless steel 304
five stages, builtwith an operation
in stainless volume
steel 304 withofan60operation
L which volume
operatesofcontinuously
60 L which
(Figure
operates1).continuously (Figure 1).
The
The information
informationabove
abovehas
hasled
ledusustotoapply
applythis distillation
this process
distillation in tequila
process production,
in tequila since
production, it has
since it
ahas
great potential for application in the tequila industry. This study aims to produce higher
a great potential for application in the tequila industry. This study aims to produce higher productivity
and energy savings
productivity whilesavings
and energy preserving
while thepreserving
tequila aroma.
the tequila aroma.
In
In this study, we evaluate the composition distilled
this study, we evaluate the composition of the fractions obtained
of the distilled fractions during the rectification
obtained during the
process by continuous
rectification process bydistillation
continuousof the ordinario
distillation obtained
of the at obtained
ordinario the industrial
at thelevel, in order
industrial to in
level, know
orderif
this distillation system allows tequila with the quality specified in the Official Standard
to know if this distillation system allows tequila with the quality specified in the Official Standardfor tequila to
be
forobtained.
tequila to be obtained.
2. Materials and
2. Materials and Methods
Methods
Alcoholic Content
100 Alcoholic Content
(% Vol.)
100
(% Vol.)
50
50
Ethanol
0
Ethanol
0 1 2 3 4 5
1 2 Fraction3 4 5
Fraction
Figure 3. Alcoholic degree of the distilled fractions obtained in the continuous distillation.
Figure 3. Alcoholic degree of the distilled fractions obtained in the continuous distillation.
3.2. Chromatographic Characterization
3.2. Chromatographic Characterization
3.2. Chromatographic Characterization
3.2.1. Content of Higher Alcohols and Aldehydes
3.2.1. Content of Higher Alcohols and Aldehydes
3.2.1.The
Content
five ofaccumulated
Higher Alcohols and Aldehydes
fractions of distillate obtained in the continuous distillation process
showedThe five accumulated
statistically fractions
significant of distillate
differences among obtained in the continuous
themselves thedistillation
ofprocess showed
The five accumulated fractions of distillate obtained regarding content
in the continuous aldehydes
distillation and
process
statistically
higher significant differences among themselves regarding the content of aldehydes and higher
showedalcohols, withsignificant
statistically fraction 1 differences
showing the highest
among amount of
themselves higher alcohols
regarding andof
the content aldehydes,
aldehydeswith
and
alcohols,
an averagewith fraction
content of 1253.66
showing
± the highest
86.51 and amount
2.87 ± 1.02 ofmg/100
higher mL
alcohols
of and aldehydes,
anhydrous with
alcohol, an average
respectively
higher alcohols, with fraction 1 showing the highest amount of higher alcohols and aldehydes, with
content4).
(Figure of 253.66 ± 86.51ofand 2.87 ± 1.02 mg/1004b), mL of anhydrous alcohol,compound,
respectivelymay(Figure 4).
an averageThe variation
content of 253.66acetaldehyde
± 86.51 and(Figure
2.87 ± 1.02 which
mg/100is mL
a very volatile
of anhydrous be due
alcohol, respectively
The
to variation
changes of acetaldehyde (Figure 4b), which
due tois a very volatile that
compound, may be in due to changes
(Figure 4). in the
The temperature
variation of the process
of acetaldehyde (Figure the
4b), equipment
which was operated
is a very volatile compound, manual
may bemode.
due
in the temperature of the process due to the equipment that was operated in manual mode.
to changes in the temperature of the process due to the equipment that was operated in manual mode.
600.0
800.0 60.0
40.0
mL mL
mL mL
400.0
600.0 40.0
20.0
mg/100
200.0
mg/100
400.0
0.0 20.0
0.0
mg/100
200.0
mg/100
Figure 4. Concentration of higher alcohols (a) and aldehydes (b) in different collected fractions.
Fraction 1 obtained in the continuous distillation system was equivalent to heads in the batch
distillation and could be removed to obtain a final product with a better aromatic profile.
Processes 2019, 7, x FOR PEER REVIEW 5 of 8
Fraction
Processes 1 obtained
2019, 7, 283 in the continuous distillation system was equivalent to heads in the batch
5 of 8
distillation and could be removed to obtain a final product with a better aromatic profile.
3.2.2. Content
ContentofofMethanol,
Methanol, Esters,
Esters, and
and Furfural
Furfural
The four
fouraccumulated
accumulatedfractions
fractions2, 3,
2, 4,3,and 5 (F2345)
4, and of distillate
5 (F2345) obtained
of distillate in the distillation
obtained process
in the distillation
did not show statistically significant differences with a 95% confidence level. An average
process did not show statistically significant differences with a 95% confidence level. An average concentration
of 95.17 ± 4.59,of11.67
concentration 95.17± ±3.56,
4.59,and 1.18± ±3.56,
11.67 0.35and
mg/100
1.18 mL of anhydrous
± 0.35 mg/100 mLalcohol was determined
of anhydrous for
alcohol was
methanol,
determinedesters, and furfural,
for methanol, respectively
esters, and furfural, (Figure 5).
respectively (Figure 5).
Volatile Compounds
140.0
mg/100 mL a.a.
120.0
100.0
80.0
60.0
40.0
20.0
0.0
1 2 3 4 5 F2345
Fraction
The
The final
final distillate
distillate obtained, which consisted
obtained, which consisted of
of the
the mixture
mixture of
of fractions
fractions 2,
2, 3,
3, 4,
4, and
and 55 (F2345),
(F2345),
was below the maximum permissible limits regarding the content of methanol, higher
was below the maximum permissible limits regarding the content of methanol, higher alcohols, alcohols, esters,
and aldehydes
esters, established
and aldehydes by thebyOfficial
established Mexican
the Official Standard
Mexican for Tequila
Standard (NOM-006-SCFI-2012)
for Tequila (NOM-006-SCFI-2012) [3]
(Table 1).
[3] (Table 1).
1. Results
TableTable of the of
1. Results major volatile
the major profileprofile
volatile for theforfinal
thedistillate obtained
final distillate by continuous
obtained distillation.
by continuous
Mean concentration ofdistillation.
Continuous Distillation NOM-006-SCFI-2012
Compound
(Σ
Mean concentration of Continuous Distillation mg/100
Fractions 2, 3, 4 and 5).mg/100 mL of a. a. mL of a. a.
NOM-006-SCFI-2012
Compound
Aldehydes 3, 4 ±and
(Σ Fractions 2,2.87 1.025).mg/100 mL of a. a. 40 mL of a. a.
mg/100
Methanol
Aldehydes 95.17 ± 4.59
2.87 ± 1.02 300 40
Esters
Methanol 11.67 ± 3.56
95.17 ± 4.59 200 300
Higher
Estersalcohols 253.66 ± 86.51
11.67 ± 3.56 500 200
Furfural 1.18 ± 0.35 4
Higher alcohols 253.66 ± 86.51 500
Furfural 1.18 ± 0.35 4
Different authors have reported the concentration increase of several compounds during
Different
distillation [5], authors havethis
while with reported
processthe concentration
(Table increase
1), the content of several
of methanol andcompounds during
higher alcohols is
distillation [5], while with this process (Table 1), the content of methanol and higher
maintained below the limits established by the Mexican regulation of tequila [3]. In addition to alcohols is
maintained
reducing thebelow
energythe limits established
consumption, multipleby the Mexican
options regulation
are generated of tequila
by being [3]. the
able to mix In addition to
fractions of
reducingtothe
interest energy
reduce consumption,
methanol contentsmultiple optionsalcohols
and/or higher are generated by being
at the end of the able to mix
process the 2).
(Table fractions
of interest to reduce methanol contents and/or higher alcohols at the end of the process (Table 2).
Processes 2019, 7, 283 6 of 8
4. Conclusions
The tequila obtained from the rectification process in this new continuous horizontal distillation
process complies with the content of major volatiles (methanol and higher alcohols) regulated by the
Official Mexican Standard. The five accumulated fractions of distillate obtained in the continuous
distillation process did not show statistically significant differences with a 95% confidence level
(p-value > 0.05) with respect to the content of methanol, esters, and furfural. However, these fractions
showed statistically significant differences with a 95% confidence level (p-value < 0.05) among
themselves regarding the content of aldehydes and higher alcohols, with the fraction of 1 being the one
that showed the highest amount of both groups of compounds.
Continuous horizontal distillation constitutes a potential alternative for the distillation of tequila
with the benefit of energy savings of 50% compared to the traditional process and the potential control
of the compounds regulated by the Official Mexican Specification for tequila.
Author Contributions: P.-d.l.R.J.D. and P.-R.R. directed the research, E.-E.M. and P.-d.l.R.J.D. supported work in
the redaction and reviewed the paper, and R.-P.M. realized the experimentation.
Funding: This research received no external funding.
Acknowledgments: We acknowledge CIATEJ for the facilities and support during the development of the present
work; Tequila San Matías Inc., from the state of Jalisco, for providing the ordinary tequila; and Tec. Abiel Alba and
Ing. Ernesto Rodríguez for the technical support during the development of the experiment.
Conflicts of Interest: The authors declare no conflict of interest.
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